RP-HPLC法测定复方消银颗粒中没食子酸、黄芩苷和黄芩素的含量

目的：建立RP-HPLC法同时测定复方消银颗粒中没食子酸、黄芩苷和黄芩素3个化学成分含量。方法：采用Shim-pack ODS（250 mm×4.6 mm，5 μm）色谱柱，以乙腈（A）-0.1%磷酸水溶液（B）为流动相，梯度洗脱（0~22 min，3% A→10% A；22~35 min，10% A→35% A；35~50 min，35% A→28% A），流速1.0 mL·min^-1，检测波长为280 nm，柱温35℃。结果：没食子酸、黄芩苷和黄芩素质量浓度分别在3.57~49.98 μg·mL^-1（r=0.999 5）、4.032~40.32 μg·mL^-1（r=0.999 4）和3.278~16.390 μg·mL^-1（r=0.999 3）范围内呈良好线性关系，平均回收率在98.74%~100.1%范围内，RSD在0.49%~1.5%范围内；3批样品中没食子酸、黄芩苷和黄芩素含量分别为0.153~0.154、0.256~0.258、0.113~0.114 mg·g^-1。结论：本方法可为复方消银颗粒多指标质量评价及控制提供科学依据。

Objective: To establish an RP-HPLC method for simultaneous determination of three components(gallic acid,baicalin and baicalein) in compound Xiaoying granules.Methods: The samples were separated on a Shim-pack ODS column(250 mm×4.6 mm,5 μm) by gradient elution with acetonitrile(A) -0.1% phosphoric acid aqueous solution(B) (0-22 min,3%A→10%A;22-35 min,10%A→35%A;35-50 min,35%A→28%A) at a flow rate of 1.0 mL·min^-1.The detection wavelength was set at 280 nm.The column temperature was maintained at 35℃.Results: The calibration curves of gallic acid,baicalin and baicalein were in good linearity over the ranges of 3.57-49.98 μg·mL^-1(r=0.999 5),4.032-40.32 μg·mL^-1(r=0.999 4) and 3.278-16.390 μg·mL^-1(r=0.999 3),respectively;their average recoveries were 98.74%-100.1% with RSD values of 0.49%-1.5%.The contents of the above-mentioned compounds in samples were 0.153-0.154 mg·g^-1,0.256-0.258 mg·g^-1 and 0.113-0.114 mg·g^-1,respectively.Conclusion: The method could be used for the comprehensive quality control of compound Xiaoying granules.